And benjamin h



Jan. 27, 1931. R. H. ADAMS ET AL METHOD OF MKING LINSEED OIL Filed July3, 1925 2 Sheets-Sheet 1 1Min FIFA-'L Lik,

ATTORNEYS.

Jan. 27, 1931. R. H. ADAMsET AL 1,790,494

' IETHOD 0F MAKING LINSEED OIL Filed July 3, 1925 2 Sheets-Sheet 2 l anPatented Jan. 2.7, 1931 UNIT-En STATI-:se

PATENT y OFFICE ROBERT n. ADAMS, or CmEENwICH,r CONNECTICUT, ANDBENJAMIN n. THUBNAN, or TUCxAHoE, NEW Yonx, assleNoEs To GOLD DUSTCORPORATION, or NEW Yonx,

N'. Y., CORPORATION 0F NEW JERSEY METHOD OF MARIN G LINSEED OIL'-Application led July 8, 1925. Serial No. 41,275.

Our invention relates to method of making linseed oil. y

Amongfthe many uses to which linseed oil is put in the arts are. two,namely, for varvery high-grade product. The ideal oil for these purposesmust be 'of light color and is preferably brilliant without any bloom.

Such an oil must also be free from vhat is v '10 known in the art asbreak when heated to a temperature substantially higher thlan525 F. orwhen cooled to say 32 F. These breaks in the ordinary oil are-.evidencedby a precipitate which will not be re-dissolved upon cooling from thehigher temperature or upon warming from th lower temperature. Thepresence of these precipitates in the oils as heretofore made, makes itnecessary for the varnish or other paint maker to age and filter 2o theoil before using it. The ideal oil shouldv a high viscosity and shouldhave quick body-A ing` nropertiesfwithwhich a larger amountofthinner'ma-v vlee used than oils as lhereto fore made. Such an oilshould yalso have a low phosphorus content, preferably less than onetWb-thousandth-of one percent. The low phosphorus content assures theformation'of v .phosphatides during the process of manufacturingproducts in which the oilv is used. Such an oil should also be of suchcharacter that upon heat bleaching the color will be suiliciently lightfor use in the' manufacture of Varmsh or m Zmc or lead grmdmg' terial instorage, as well as vthe storage space Preferably there should be nonecessity for refining the oil bythe use of caustics, acids,

or other chemicals.

Linseed oil as heretofore made has had certain defects which it has beenimpossible to overcome prior to our invention. Two of the greatestdefects have been the color and the` breaks uponheating to 525 F. orhigher, and upon cooling to 70 F. or lower. So far as we are advised noone prior to our invention has disclosed how these defects maybeovercome without at the same time creating other defects somewhat lessobjectionable, but

- oil.

Efforts have been made heretofore to over- .come the objectionable colorof the oil by 3 nilshes and zinc grinding which require ay treating thesame with various chemicals, such as alkalies, acids, and others, andwhile this treatment hasbeensuccessful to a certain extent as to color,these .chemicals have so affected the structure or composition of theoil that the oil breaks whencooled, as above explained. The precipitateresulting fromrthe breaks renders it necessary for the consumer of the'oil to allow the same to remain in storage ordinarily for a period ofsix months. During this period the temperature of the oil changesaccording to the seasons and the precipitate settles in the barrels orother containers. When it is desired to use the oil it is then passedthrough a filter to remove this precipitate and clarify the oil. If itwere attempted to use the oil before this aging period, theseprecipitates would be formed in the oil after the same had been madeinto varnish or other paints with the result that the paint or varnishwould be objectionable and in fact unusable on high-class jobs.Itthe-refore becomes necessary that the oil be stored' to allow theprecipitate'to form and settle.

4Some varnish manufacturers have installed -refrigerating apparatus to.carry the oil and other equipmentnecessary therefor. The art hastherefore been seeking for some time a solution of this diiiiculty whichwill relieve it of the dilemma of either storing the oil or of using thesame withthe chance that the product made therefrom will be defectivebecause lof the precipitated matter. 'We have made certain discoveriesand have devised a process of making a linseed oil free from all thedefects above set forth and an oil which is superior to the best agedoil exist-l ing heretofore and an oil which may be used immediately uponproduction without the V100 necessity for any chemical treatmentwhatever, and at a lower cost than the best oils as heretofore made.

We have discovered that one of the chief causes of defects to the oil asheretofore made i's the action of the constituents of the foreign matterwhich is invariably mixed with the flaxseed from which the oil isextracted. This foreign material is usually designated as dockageandconsists of seeds of wild mustard, foxtail, vetch, white mustard, falseflax, pig- Weed, clover and grass; also dust, grit` chaff, etc. Ofcourse this doekage Willcontain other material and seeds of other plantsdependino upon the section of the country or world 2from which the seedsare gathered. Another substantial cause of the defects in the oil asheretofore made, was that of' improperly controlled heat during theextraction of the oil from the seeds. We have discovered that ifthoroughly cleanfiaxseeds are treated as heretofore wherein thetemperature is not limited to below about 11.0 F., the resulting oil hasmost of the defects above mentioned. One of the chief defects is thebreak uponvheating. On the other hand, it makes no difference whatmethod is used to extract the oil from the seed, if the seeds have notbeen ,previously cleaned, the above-mentioned defects will appear.

Our new process consists in first cleaning the seeds of dockage so thatthere will'remain in the seeds preferably not`more than 1% to 11/270,preferably the former, of dockage. These seeds are then placed in anexpeller and the oil expelled therefrom by cold pressing.A

That is to say, the expulsion of the oil is so regulated that thetemperature of the oil running from the screen to the drip-pan isbetween 90 and 100 degrees F. Ordinarily this operation results in theexpulsion of about. 45 to 50% of the oil content of the seeds Withinthel temperature range above given. The cake .from which this oil hasbeen expelled is then treated by an hydraulic press operation in anyknown Way to remove the balance of the oil. The oil coming from theexpellers may contain slight traces of moisture and fine particles ofmeal. In order to remove this material a. quantity of the oil is runinto and fills a tank of about five to six barrels capacity. To thisabout 100 pounds of diatomaceous earth is added and the mixture isthoroughly agitated with air. This mixture is then run into a filterpress. This small quantit)7 mixed with the diatomaceous earth causes theformation of a filter layer on the filter units and then a lar'gequantity of the untreated oil may be run throughlthe filters, whichassures a very clear and brilliant oil. This oil after filtering showsabout .60 acid number. color 50 yellow, 5.3 red. This oil as it comesfrom the filter has many uses and is particularly useful in themanufacture of varnish and is equal in color and other properties to thebest varnish oil on the market'which has been chemically treated andbleached. This oil is given in the table below as TA oil.

The oil from the filter may be treated in a very simple manner, thatisf-to say, by heat oil described at the beginning of thisspecification, having all of the qualities there mentioned without anydefects, and in the table below is designated as P. M. P. oil.

We have noted that When'oil made by ordinary methods is chilled to 60 F.or lower a cloudiness sometimes appears'and does not disappear until theoil is at a temperature higher than that at which tlfe lcloudinessappeared. But with our oil a cloudiness does not appear until thetemperature is 32 F.

"or lower. When a cloudiness appears, it will disappear before thetemperature rises to 48 F., indicating that any suspended matter (suchasglycerides crystallized out) caused by the chilling is soluble in theoil at the teinperature of 48 F. or lower.

This bleached oil has a third use and that is that of makingslight fattyacids. These fatty acids-are usually used for makingdriers or salts ofdrier metals. They are also used for increasing the acid content of anyoil used in either zinc-grinding or lead-grinding. Such acids, as madefrom ordinary linseed oil, either raw or refined, have the greatdisadvantage of being of a dark color. This is objectionable ifit isdesired to use the acids to increase the acid content of a grinding 011,because of a tendency to discolor the product. By employing the bleachedoil of our process fatty acid may be made of light color. When used toincrease the acid content of an oil, thesefatty acids may be merelyadded to rthe oil without treating the total quantity of oil as isusually done by the addition of sulphuric acid, heating and bleaching,which operation obviously consumes considerable time, and is ratherexpensive. Even if this expensive method is used, the resulting oil ismany times darker in color than that made from the use of fatty acidswhich were made from our bleached oil.

tirely free from suspended colloidal matter` or precipitates which arenot readily soluble 'in the material upon change ot' temperature:v thematerial does not break when heated to a high /t/emperatureor cooled toa low temperature;- has a high viscosity and quick bodying properties;requires no refining by chemicals 4and therefore contains substantiallyall of its {atural constituents; has a lowphosphorus content; willproduce fatty acids of unusually light color and may be used as avarnish oil or as a grinding oil in the production of the highest gradepaint products.

In the accompanying drawings, we have indicated in: Fig. 1 a fiow sheetgivingl a diagrammatic representation of apparatus. which we have usedin the process above dethis apparatus'is by no means vthe only apparatuswhich may be -used in our process,

but that Yit is merely representative.- We have sh wn in Fig. 2 anenlarged view of 1a seed cleaning machine somewhat in detai I' In Fig. 3we have shown a view of' the ex- J peller on a larger scale than'thatshown in Fig. 1.

Our invention will be better understood by reading the' followingdescription of the drawings. forming a part thereof.

Referring to Fig. 1, the apparatus consistsl of a bin l for seedstorage.` The seeds are conducted from the bin 1 to the seed cleaners 2,3 and 4. In treating flaxseed we have found I what is known in the tradeas a No.8 Monitor cleaner, made by the Huntley Manufacturing, Company ofSilver Creek, N. Y., very effec#vv tive for our purpose. The cleaners 2and 3 are of the type above indicated and each is 40 provided w1th a16x21/2 inch wire screen and a 4/64V ofan inch perforated metal screenfor mustard seed fraction ofthe dockage. By running the seed over thesecleaners the dockage is reduced to about 1.6 per cent. The

4 5 cleaner 4 is what is known in the trade as a No. 6 Monitor` cleaner.This cleaner4 is provided with a mustard screen made up of a.

metal plate perforated to 4/64 of an inch.

t When the seeds are run over this cleaner they,

are cleaned of dockage down to about 1 per cent'or less.

Connected with each ofthe cleaners above described is a dust collector5, 6 and 7, respectively. After the seed has passed over these threecleaners it is conveyed into a Y hopper 8. The rough dockage isdischarged at 9 and the mustard seed fraction of the..

J dockage at 10. v

The clean seeds are' conveyed fro' 1 the hopper 8 into the cracking orfiaking r achine 11'.

(This is a two-high roll machine wi h the rolls so adjusted as to justfiake or crack the hulls without grinding the hulls with the meats. Thismachine is driven at a speed ofabout 6;.y 180 R. P. M. andis providedwith means for adjusting the rolls to regulate the crackin From thismachine the cracked or flaked see s are delivered to the mixer 12 inwhich moisture is mixed with the seeds tothe extent of about-3 per cent.An agitating means 13 is 70' shown for insuring a thorough mixing.. Thevseeds mixed with this moisture areconducted by screw conveyor 14 to theexpellers. The pressingequipment consists of a plate press 15, a boxpress-16 and a standard expeller 17. 75 By ordinary manipulation thesepressers are operated so as to iex elfrom the seeds about 45 to 50 percent o the oil without raising the temperature of the oil as it leavesthe expellers to a point higher than 90 to 110 F; The oilis conveyedfrom the expellers to a,

t scale tank 18 where the oil is weighed. Five scribed. .We wish it tobe understood that with about 100, pounds of a certain filter aid,

. such as diatomaceous earth. The oil and filter aid are thoroughlymixed by air agitation and the mixture is then run into the filter press20, whereupon the' filter aid forms a coating on the filter elements,thus assuring a co1 plete filtering of the oil which is later r nAthrough. From the filter press the oilis runinto testing tanks 21 and 22and is there tested for .quality before being delivered to the storagetank 23. z

The test of thev oil in the tanks 21 and 22 consists in'removing asample from the tank and testing the acid number and the color of theoil., In our operation the .acid number runs between .58 and .6 and thecolor from about 50 yellowand 7 red to about -35 yellow, 57.35 red. Thecolor measurements herein given were determined by the Lovibondcolorimeter with 5% inch columr and used inthe customary manner.

. The 'oil that is delivered to the tank 23- 'has many uses, asexplained in the first part 'of this specification, but for manypurposes we find it advisable to further treat the oil by passing itinto the bleaching tank 24,. in which is placed an agitator 25. A steampipe 26 is placed in the bleach tank and by means of steam thetemperature of the oil in the tank 24 may be controlled to any desiredpoint. We prefer to maintain the -temperature 1n the tank 24 at about180 F.

We prefer to add to the oil in the tank 24 about 31/2 per cent fullersearth and of 1 per cent of a suitable carbon bleaching material.v Afterthe addition ofthe earth and` the bleaching material the oil is pumpedthrough the filter press 27. At the beginning of the operation it iscustomary to return the oil from the filter press to the bleaching tanknntil a sufficient bed or cake of filter material is built up on thepress units. After the filter press is properly prepared the oil is runcontinuously from the filter press into a storage tank' 28. Theoilcomigfrom the filter press 130 Y 27 has a color ranging from about 10yellow and 1 red, to about 20 yellow and 2 red, and an acid numberofabout .5.

We have shown in Fig. 2 a somewhat more detailed view of the seedcleaning machine. This machine per se forms no part of our invention andwe therefore do not deem it necessary to fully illustrate and describethe same. The machine consists of a framework 29 supporting a series ofscreens 30, 31, 32, 33. These screens are reciprocated by eccentrics 34and 35 on a shaft 36. The material .to be cleaned is introduced throughthe receptacle 37 at one end of the machine or receptacle 38 at theother, or bothat the same time. The foreign matter is removed by meansof the fan 29 and the cleaned flax seeds are delivered at 40. Themustard seeds-are delivered at 41, and the screenings at 42. Thismachine is well known in the art and its operation is thoroughlyfamiliar to those acquainted with the cleaning of axseed..

In Fig. 3 we have shown a standard expeller which is operated by motor43 and acts to expel the oil from the cracked flaxseed by compressingthe seed between the plates 44. The oil is delivered at 45 and the cakeor solid matter may be discharged at 46 from the expeller in awell-known manner. This machine is'also Well known to those skilled inthe art and its construction and operation need no further description.

The following table gives the ranges of values of the various physicalcharacteristics of crude oil made in the ordinary way and of the oil asit comes from the tank 23 (TA oil) and ofthe oil in the tank 28 P. M. P.011). Oil s Raw Color 300 yellow, 22 red Acld No 0.6 to 4.0 Viscosity11/2 seconds Iodine No 180 to 198 Grav1ty .932 to .934 F. F. A .3% to2.0% Unsapomfiable matter Not over 1.50%

Oil Color AcidNo. Viscosity Iodine No. Gravity :ey-5.311 TA to .6 to 1lnesc' 18o zo 198 .932 m .934

10i/ 1R PMP to .6 to 1 llfesc' 180 to 198 .932 to .934

Unsa- Refrac- Bodylng pom- Phosphorus O11 F' F' A' igx rate able contentmatter TA .3 to .5 1. 4793 1 to 5 hrs. 1.07 Less than 001 PMP 3 to 5 1.4792 1 to 4 hrs. 76 Less than 002 While we have given detailssuch -asthe Achanges may be lnade and satisfactory results produced, but we havefound that the method above described in detail is the preferredcommercial method and that the product identified above is entirlysuitable for all commercial purposes.

Throughout the specification and claims the term viscosity and thevalues thereof given or indicated, are determined by the bubble method,as follows: The instrulnent consists of a glass tube 6 long by indiameter. The tube is sealed at one end and is made in the form of ahomeopathic vial so that it can be almost filled with oil or othermaterial and Sealed at the open end with a cork stopper. The tube isfilled with oil or other material to such an extent that when thestopper is inserted the air bubble when allowed to flow along the sideof the tube is 1/3 the diameter of the tube, i. e. it is 1A, indiameter. The viscosity is determined by first bringing the air bubblecompletely to method of treatment to a slight degree depending upon thecharacter of the seed used and the section of the country or world fromwhich the seeds came, but in view of the foregoing disclosure,y webelieve that those skilled in the art can easily and readily adapt theprocess to the treatment of any seeds by very slight experimentation.

We claim:

1. The method of extracting linseed oil which consists in cleaning thewhole uncracked axseed to a maximum of about 1.5% dockage and pressingthe oil from the cracked flaXseed while limiting the upper temperatureof the oil below F.

2. The method of extracting linseed oil which consists in cleaning thewhole unmg su stantially 110 F.

R. H.. ADAMS. BENJAMIN'H. THURMAN.

